正交试验在中药材微量元素测定前处理研究中的应用

目的: 采用国家有证标准物质黄芪、黄豆、茶叶,应用正交试验建立药材中元素测定的微波消解方法。 方法: 采用正交试验对电感耦合等离子体质谱法和原子荧光法测定药材中Cr、Ni、Cu、As、Hg、Cd、Pb 7种重金属及有害元素含量的前处理微波消解方法的参数进行优选,以标准物质中各元素的标准范围值的中值为基数,相对于基数的偏离程度设计出评分方案,据此计算出考察指标。 结果: 消解溶剂、消解温度、消解时间、赶酸程度四因素对不同元素的测定有不同的影响。 结论: 本法用标准物质的标准值作为优选最佳消解参数试验条件的依据,大大提高了实验结果的准确性。对同时消解不同部位的药材及同时测定多个微量元素具有一定的参考价值。

Objective: To establish an effective microwave digestion method for determination of the elements in traditional Chinese medicine(TCM)by orthogonal design with certified reference materials(CRM)of Astragali Radix,soybean and tea. Methods: The parameters of microwave digested in sample preparation for determination of 7 heavy metals and toxic elements(Cr,Ni,Cu,As,Hg,Cd,Pb)in TCM by inductively coupled plasma mass spectrometry(ICP-MS)and atomic fluorescence spectrometry(AFS)were optimized by orthogonal design,which based on the basis of median of standard range of CRM and an evaluation plan was designed to calculate the index of examination. Results: Digestion solvent,digestion temperature,digestion time and acid evaporation could affect the determination of different elements. Conclusion: The method based on the characteristic value of CRM from optimization of best tests,greatly improves the accuracy of test results.It has a certain reference value for digestion of parts of TCM and simultaneously determination of trace elements.

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